铜藻岩藻黄素提取及纯化工艺研究

为了对岩藻黄素的提取、纯化进行系统研究，进而为高纯度岩藻黄素的工业化生产提供研究基础，筛选了适用于提取铜藻（Sargassum horneri）鲜藻中岩藻黄素的有机溶剂，并通过单因素实验和正交实验确定了最佳的提取溶剂浓度、提取温度、提取时间、料液比等工艺参数。随后采用硅胶柱层析法进行纯化，并通过单因素实验确定了最佳的硅胶柱床高度、上样量和洗脱流速。最后采用制备液相法对经层析纯化的岩藻黄素进一步纯化。结果表明，有机溶剂萃取的最佳工艺条件为：甲醇浓度90%，提取温度50 ℃，提取时间1 h，料液比1∶10，此条件下岩藻黄素提取率达到(0.258 9±0.003 6) mg·g-1鲜重（FW）［(1.078 8±0.015 0) mg·g-1干重（DW）］。硅胶柱层析的最佳工艺条件为：硅胶柱床高度10 cm，上样量6 g，洗脱流速10 mL·min-1，此条件下岩藻黄素得率为0.176 5 mg·g-1FW（0.735 3 mg·g-1 DW），纯度为87.01%±0.88%。经制备液相进一步纯化后，岩藻黄素得率为0.127 1 mg·g-1 FW（0.529 4 mg·g-1 DW），纯度为99.27%±0.22%。研究所用工艺简单，岩藻黄素得率高，为高纯度岩藻黄素的制备提供了实验基础。

Study on Extraction and Purification Technology of Fucoxanthin from Copper Algae

In order to systematically study on the extraction and purification of fucoxanthin and further provide research basis for the industrial production of high-purity fucoxanthin,an organic solvent suitable for extracting fucoxanthin from fresh copper algae(Sargassum horneri)was selected,and the optimum technological parameters including extraction solvent concentration,extraction temperature,extraction time,solid-liquid ratio were determined through single factor and orthogonal experiments.Subsequently,silica gel column chromatography was used for purification,and the optimum silica gel column bed height,sample loading amount and elution flow rate were determined through single factor experiments.Finally,the fucoxanthin purified by silica gel column chromatography was further purified by preparative liquid chromatography.The results showed that the optimum process conditions for organic solvent extraction were as follows:methanol concentration 90%,extraction temperature 50℃,extraction time 1 h,and solid-liquid ratio 1∶10.Under these conditions,the extraction rate of fucoxanthin reached(0.2589±0.0036)mg·g-1 fresh weight(FW)(1.0788±0.0150)mg·g-1 dry weight(DW)].The optimum technological conditions for silica gel column chromatography were as follows:the height of silica gel column bed was 10 cm,the loading amount was 6 g,and the elution flow rate was 10 mL·min-1.Under these conditions,the yield of fucoxanthin was 0.1765 mg·g-1 FW(0.7353 mg·g-1 DW),and the purity was 87.01%±0.88%.After further purified by preparative liquid chromatography,the yield of fucoxanthin was 0.1271 mg·g-1 FW(0.5294 mg·g-1 DW)and the purity was 99.27%±0.22%.The research process was simple and the yield of fucoxanthin was high,which provided an experimental basis for the preparation of high purity fucoxanthin.